HPLC Determination of Aflatoxins in Tea in Bags with Extraction by Matrix Solid Phase Dispersion
摘 要
提出了基质固相分散-高效液相色谱法测定袋泡茶中黄曲霉毒素B1、B2、G1和G2含量的方法。优化的试验条件为:① 样品与分散剂(中性氧化铝)的质量比为1比4;② 洗脱剂乙腈的用量为6 mL。以Symmetry C18色谱柱为分离柱,以甲醇-水(1+1)混合液为流动相进行分离。采用荧光检测,激发波长为365 nm,发射波长为435 nm。黄曲霉毒素B1、B2、G1和G2在一定的质量浓度范围内与其峰面积呈线性关系,方法的检出限(3S/N)在0.05~0.15 μg·L-1之间,测定下限(10S/N)在0.15~0.50 μg·L-1之间。以空白样品为基体进行加标回收试验,所得回收率在88.3%~96.8%之间,测定值的相对标准偏差(n=6)在4.3%~6.8%之间。
Abstract
A method of HPLC for the determination of aflatoxins B1, B2, G1 and G2 in tea in bags with extraction by matrix solid phase dispersion was proposed. The optimized conditions found were as follows: ① mass ratio of sample to dispersant (neutral Al2O3): 1∶4;② volume of the eluant (acetonitrile) used: 6 mL. Symmetry C18 chromatographic column was used as stationary phase, and a mixture of methanol and water (1+1) was used as mobile phase in the separation. Fluorescence detection at the wavelengths of (λex) 365 nm and (λem) 435 nm was adopted in the determination. Linear relationships between values of peak area and mass concentration of aflatoxins B1, B2, G1 and G2 were kept in definite ranges, with detection limits (3S/N) in the range of 0.05-0.15 μg·L-1 and lower limits of determination (10S/N) in the range of 0.15-0.50 μg·L-1. On the base of blank sample, test for recovery was made by standard addition method;values of recovery found were in the range of 88.3%-96.8%, with RSD′s (n=6) in the range of 4.3%-6.8%.
中图分类号 O652.63
所属栏目 工作简报
基金项目 宁夏自然科学基金资助项目(NZ14226)
收稿日期 2013/11/22
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备注徐飞(1983-),男,江苏赣榆人,检验师,硕士,主要从事食品安全与农药残留分析研究。
引用该论文: XU Fei,GAO Gui-tao,QIAN Xin. HPLC Determination of Aflatoxins in Tea in Bags with Extraction by Matrix Solid Phase Dispersion[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2014, 50(11): 1390~1393
徐飞,高贵桃,钱鑫. 基质固相分散-高效液相色谱法测定袋泡茶中黄曲霉毒素[J]. 理化检验-化学分册, 2014, 50(11): 1390~1393
被引情况:
【1】谢昕,李红艳, "免疫亲和柱净化-光化学柱后衍生-高效液相色谱法测定柏子仁中的黄曲霉毒素",理化检验-化学分册 52, 541-544(2016)
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参考文献
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【13】王炼,黎源倩,王海波,等.基质固相分散-超高效液相色谱-串联质谱法同时测定畜禽肉和牛奶中20种兽药残留[J].分析化学, 2011,39(2):203-207.
【2】KOLOSOVA A Y, SHIM W B, YANG Z Y, et al. Direct competitive ELISA based on a monoclonal antibody for detection of aflatoxin B1. Stabilization of ELISA kit components and application to grain samples[J]. Anal Bioanal Chem, 2006,384(1):286-294.
【3】张鹏,赵卫东,张艺兵.高效薄层色谱法测定黄曲霉毒素B1、B2、G1、G2[J].分析化学, 2000,28(3):392-392.
【4】TUDORACHE M, BALA C. Sensitive aflatoxin B1 determination using a magnetic particles-based enzyme-linked immunosorbent assay[J]. Sensors, 2008,8(12),7571-7580.
【5】宋慧君,马惠蕊,裴轶君,等.黄曲霉毒素B1液相芯片定量检测方法的探索[J].农药学学报, 2011,13(4):394-401.
【6】李佐卿,章再婷,谢东华,等.免疫亲和柱高效液相色谱法快速测定牛奶和奶粉中黄曲霉毒素M1、B1、B2、G1、G2[J].理化检验-化学分册, 2005,41(6):406-408.
【7】毕瑞峰,谢志先,付萌.高效液相色谱-串联质谱法检测腰果中的黄曲霉毒素[J].色谱, 2011,29(12):1155-1159.
【8】马良,张宇昊,李培武.LIF-HPCE法检测食品中的黄曲霉毒素B1[J].食品科学, 2009,30(10):135-139.
【9】BARKER S A. Matrix solid-phase dispersion[J]. J Chromatogr A, 2000,885:115-127.
【10】SHI Xiao-lei, LI Xun-wen, LIU Jing-bo, et al. Lignan ebtraction from the roots of sinopodophyllum emodi wall by matrix solid-phase dispersion[J]. Chromatographia, 2010,72:713-717.
【11】OZOWICKA B, JANKOWSKA M, RUTKOWSKA E, et al. Comparison of extraction techniques by matrix solid phase dispersion and liquid-liquid for screening 150 pesticides from soil, and determination by gas chromatography[J]. Pol J Environ Stud, 2012,21(4):973-992.
【12】郑萍,盛旋,余晓峰,等.基质固相分散液相色谱法检测辣椒产品中的黄曲霉毒素[J].色谱, 2006,24(1):62-64.
【13】王炼,黎源倩,王海波,等.基质固相分散-超高效液相色谱-串联质谱法同时测定畜禽肉和牛奶中20种兽药残留[J].分析化学, 2011,39(2):203-207.
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